Hydrochloric Acid → HCID 11439106, compound

HRID 431278Notes

Reaction equation

HRID 431278 reaction equation
[F:1][C:2]1[CH:3]=[CH:4][C:5]([OH:12])=[C:6]([S:8]([OH:11])(=[O:10])=[O:9])[CH:7]=1.Cl[Si:14]([CH3:17])([CH3:16])[CH3:15].Cl>>[F:1][C:2]1[CH:3]=[CH:4][C:5]([O:12][Si:14]([CH3:17])([CH3:16])[CH3:15])=[C:6]([S:8]([O:11][Si:14]([CH3:17])([CH3:16])[CH3:15])(=[O:10])=[O:9])[CH:7]=1

Participants

4

Reactant 3

HCID 313Hydrochloric AcidHCID 6397Chlorotrimethylsilane2×HCID 11480951HCID 11480951, compound

Product 1

HCID 11439106HCID 11439106, compound

Procedure

302 g (1.57 mol) of 5-fluoro-2-hydroxybenzenesulfonic acid are admixed, under an inert gas atmosphere at room temperature with stirring, with 794 ml (683 g, 6.28 mol) of chlorotrimethylsilane, and the mixture is heated to boiling. After the vigorous release of HCl has died down, a further 794 ml of chlorotrimethylsilane are added and the turbid solution is heated under reflux for 96 hours. After cooling, the precipitate is filtered off under inert gas, the excess chlorotrimethylsilane is removed at 40-50° C. under slightly reduced pressure (about 4000 Pa) and the product is obtained by fractional distillation in vacuo.

Workup

  1. customare admixed, under an inert gas atmosphere at room temperature
  2. temperaturethe mixture is heated to boiling
  3. temperaturethe turbid solution is heated
  4. temperatureunder reflux for 96 hours
  5. temperatureAfter cooling
  6. filtrationthe precipitate is filtered off under inert gas
  7. customthe excess chlorotrimethylsilane is removed at 40-50° C. under slightly reduced pressure (about 4000 Pa)
  8. customthe product is obtained by fractional distillation in vacuo

Sources & evidence

ORD record
ord-a00aff52677b443cab12385bbc2e41fa
Source dataset
uspto-grants-2003_12
Patent number
US06657072B2

Reaction notes

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